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Synthetic method of 3-chloro-2-methylaniline

A synthesis method, the technology of methylaniline, applied in the field of synthesis of 3-chloro-2-methylaniline, can solve the problems of catalyst poisoning, high product cost, poor activation performance, etc., and achieve low production cost and high safety , The effect of high product yield

Inactive Publication Date: 2011-11-09
山东福尔有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this method is that the catalyst is easily poisoned, the activation performance is poor, and the yield of this method can only reach 87%, and the product cost is relatively high

Method used

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  • Synthetic method of 3-chloro-2-methylaniline
  • Synthetic method of 3-chloro-2-methylaniline
  • Synthetic method of 3-chloro-2-methylaniline

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] In a 1000 ml three-neck flask equipped with mechanical stirring, reflux condenser, and thermometer, add 50 ml of water and 1 mol of sodium polysulfide to the flask, stir the mixture and add 0.4 mol of ammonium bromide, and gradually add 1 mol of 6- Chloro-2-nitrotoluene, the temperature is controlled at 30°C, and the following chemical reactions occur in the system:

[0015]

[0016] After the reaction was completed, the upper organic phase was separated, washed with water until neutral, and the organic phase was distilled at a vacuum of 0.1 MPa to collect 139.8 grams of fractions at 127-137°C.

[0017] With 3-chloro-2-methylaniline as standard, gas chromatography analysis. The analysis results are shown in Table 1 and Table 2.

[0018] Table 1.3-Chloro-2-methylaniline standard sample chromatographic analysis results

[0019] peak number

[0020] Table 2. Fraction chromatographic analysis results

[0021] peak number

[0022] The purity of 3-ch...

Embodiment 2

[0024] In a 1000ml three-neck flask equipped with mechanical stirring, reflux condenser, and thermometer, add 50ml of water and 2mol sodium polysulfide into the flask, stir the mixture system and then add 0.5mol ammonium chloride, and gradually add 1mol 6-chlorine -2-Nitrotoluene, the temperature is controlled at 105°C, and the following chemical reactions occur in the system:

[0025]

[0026] After the reaction is completed, the unreacted acid liquid in the kettle is first recovered, the upper organic phase is separated, washed with water until neutral, the organic matter is distilled, the vacuum degree is 0.1 MPa, and 140.2 grams of fractions at 127-137 ° C are collected.

[0027] With 3-chloro-2-methylaniline as standard, gas chromatography analysis. The analysis results are shown in Table 3 and Table 4.

[0028] Table 3.3-Chloro-2-methylaniline standard sample chromatographic analysis results

[0029] peak number

[0030] Table 4. Fraction chromatographic a...

Embodiment 3

[0034] In a 1000ml three-neck flask equipped with mechanical stirring, reflux condenser, and thermometer, add 50ml of water and 1mol sodium polysulfide into the flask, stir the mixture system and then add 0.6mol ammonium bisulfate, and gradually add 2mol 6-chlorine -2-Nitrotoluene, the temperature is controlled at 70°C, and the following chemical reactions occur in the system:

[0035]

[0036] After the reaction is completed, the unreacted acid liquid in the kettle is first recovered, the upper organic phase is separated, washed with water until neutral, the organic matter is distilled, the vacuum degree is 0.1 MPa, and 281 grams of fractions at 127-137 ° C are collected.

[0037] With 3-chloro-2-methylaniline as standard, gas chromatography analysis. The analysis results are shown in Table 5 and Table 6.

[0038] Table 5.3-Chloro-2-methylaniline standard sample chromatographic analysis results

[0039] peak number

[0040] Table 6. Fraction chromatographic ana...

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Abstract

The invention discloses a synthetic method of 3-chloro-2-methylaniline, which comprises the following steps: dissolving polysulfide in water, stirring, adding ammonium salts, heating, controlling the temperature to be 30-105 DEG C, adding dropwisely 6-chloro-2-nitrotoluene to perform a reaction; after the reaction, separating the organic phase, washing with water to neutrality, performing distillation of the organic phase with a vacuum degree of 0.1 MPa, collecting fractions at 127-137 DEG C to obtain 3-chloro-2-methylaniline. The synthetic method of 3-chloro-2-methylaniline of the invention has high yield, low production cost, and high security.

Description

technical field [0001] The invention relates to a synthesis method of 3-chloro-2-methylaniline. Background technique [0002] 3-Chloro-2-methylaniline can be used in the dye industry to synthesize dye DB-50, and in the pesticide industry to produce paddy field herbicide fast barnyardgrass (BAS-514H). It is also an important pesticide intermediate. In the prior art, the preparation of 3-chloro-2-methylaniline is mainly obtained by hydrogenation reduction, which is expressed as follows with a chemical reaction formula: [0003] [0004] Wherein X is one of Ni, Gr, Pt, Pd, Co, Cr and Rh. The disadvantage of this method is that the catalyst is easily poisoned, the activation performance is poor, and the yield of this method can only reach 87%, and the product cost is relatively high. Contents of the invention [0005] The purpose of this invention is to provide a kind of synthetic method of the 3-chloro-2-methylaniline with high yield, low production cost and high safety...

Claims

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Application Information

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IPC IPC(8): C07C211/52C07C209/36
Inventor 于俊田张玲孙志国王洛
Owner 山东福尔有限公司
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